Method of forming a phenolic condensation product



Patented Apr. 7, 192 5.

UNITED STATES PATENT OFFICE.

EDWIDT ROLKER, 0F BALTIMORE,

MARYLAND, ASSIGNOR TO THE PEBIATI IITE GOI- PANY, A GOPABTNEBSHIPCOMPOSED 0F GEORGE EARTH, HILTON W. GATCH, AND v EDWIN ROLKEB', ALL OFBALTIMGBE KARYLAND.

METHOD OF FORMING A PHENOLIC CONDENSATION PRODUCT.

No Drawing.

To all whom it may concern:

Be it known that I, EDWIN Rommu, a citizen of the United States,residing at Baltimore, in the State of Maryland, have invented certainnew and useful Improvements in Methods of Forming a PhenolicCondensation Product,of which the following is a specification. I

' The invention relates to an improved method of reacting withformaldehyde or its polymers upon phenol or its homologues.

Condensation products resulting from the chemical action of aldehydes onphenols have been obtained by heating phenol and formaldehyde. .VVhereno condensing agent is added, the reaction is slow, requiring heatingfor a long period of time and at high temperatures. To accelerate thereaction, condensing agents, acids or salts, have been used. Thereaction in such cases is usually vigorous and diflicult to control.Furthermore, the condensing agent, as commonly used, is introduceddirectly'nto the reacting mass and becomes intimately mixed therewith sothat it is not removable fromthe product without further treatment, if'at all. In such processes, the

base, alkali or acid-used as the condensing agent, is commonlv left inthe product. This results in impurities in the product which im ppirsits value for certain uses.

1e primary object of my invention is to provide a process of forming acondensation product which will enable the condensation 4" to beeffected on a commercial scale and in a simple, practical and rapidmanner. One of the advantages of my improved process 'is that it reuires much less time for the completion 0 the reactions than theprocesses heretofore used.

Another object of the invention is to provide a process that may beeasily controlled and that may be arrested at any desired state in orderto secure intermediate products having particular characteristics andproperties. A further object is to provide an improved condensing agentwhich may be used repeatedly and is comparatively inexpensive, and whichpossesses other distinct advantages over the condensing agentsheretofore emgloyed.

ther objects and advantages of my in- Application filed March 18,

in the form of various 1920. Serial 1W0. 886,940.

more fully in the following specification and appended claims. In ageneral way, the process consists in reacting on a phenolic body with amethylene-containing substance. A mixture of phenol or its homologuesand formaldeh do or its polymers, ular proportions required for thereaction, or approximately two volumes of phenol to one of formaldehyde.In practicing the process, I may use commercial phenol or cresol (2parts) and commercial (40%) formaldehyde (1 part). The phenolic andmethylene-containing substances and their proportions may be varied,however, without departing from my invention.

The substances are placed in a closed container to the exterior of whichheat is applied. Although of the process, an advantage is derived fromvention will appear is taken in about the mo ecnot requisite to thesuccess the employment of a double-walled or water.-

jacketed container or one which has some other means for tempering theheat to which the contents of the container are The heating is startedat a moderate temperature. In some instances, it may be desirable toincrease the temperature, to accelerate the process. the temperature beincreased, the best results being obtained by using a moderate degreevof heat, in the neighborhood of 0., and mainta' ing the temperature ofthe reacting mass approximately constant by thermostatic regulation, orotherwise.

The. heating may be done at ordinary atmospheric pressure, or at higheror lower pressures. Where porosity of the final condensation product isobjectionable and a compact and homogeneous product is desired,- anincreased pressure is advantageous. Such pressure maybe introduced intothe closed container in any suitable manner.

The reaction is induced by the application of heat to the mixture and bythemt-roduction into the mass within the container of a condensing agentof improved nature and form. The condensing agent which I subjected.

but it is not necessary-that"- employ is a basic salt, preferably ofsodium,

has been found that the basic salt and aluminum, when immersedin themixture,

act as a catalytic couple and have the elfect of distinctly acceleratingthe reaction. By the use of this catalytic couple, a more vi rous and a'quicker reaction is secured t an by any other condensingagnt, with aconsequent acceleration o e process. A further advantage of thiscatalyst as a condensing agent is that the salt, being in solid form andconfined within a holder or container having only not mix with thereacting mass to form impurities in the product. Furthermore, the saltwhich forinsan element of my catalytic agent, is not injurious to theproduct even if it should become mixed therewith. The catalyst willcontinue its action until a definite viscosvivtfi of the intermediateproduct is attained. on this sta is reached, the perforated container iswit drawn from the mass. This may be done either at or just before thedesired degree of viscosity of the mass has been arrived at, it beingpossible to arrest the reaction 'atany stage of the process by thewithdrawal of this perforated container.

To obtain the final condensation product,

1' subject the intermediate condensation product to heat and pressure.An initial air pressure of sixty pounds is preferable, accompanied b agradual increase in the temperature om that ordinarilyused to atemperature corresponding to twenty or thirty pounds steam pressure fora short period (about fifteen or twenty minutes).

minute apertures, does mediate condensation container and enclosed saltbefore the react- I 7 ing mass hardens.

2. A process of forming a phenolic intermediate condensation productcomprising mixin a phenolic body and a reactive methy ene-containingsubstance, introducing therein a condensing agent consisting of a basicsalt of sodium within a skeleton aluminum container and withdrawing saidcontainer before the reacting mass hardens. 3. A process of forming aphenolic interproduct comprising mixin a phenolic body and a reactivemethy one-containing substance, introducing therein as a condensingagent a basic salt of sodium within a skeleton container of aluminum,applying heat to the mixture, maintaining the temperature of thereacting mass.

approximately constant during the reaction,

and withdrawing the container from the mass before the masshardens.

4. A process of forming a phenolic condensation product comprisingmixing a phenolic body and a reactive methylenecontaining substance, andsubjecting the mixture to the action of a condensing agent consisting ofa basic salt and aluminum.

In testimony whereof I aflix my signature.

. EDWIN ROLKER.

